CN100542663C - A permanent magnet rotating stirring device - Google Patents
A permanent magnet rotating stirring device Download PDFInfo
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- CN100542663C CN100542663C CNB2006101695554A CN200610169555A CN100542663C CN 100542663 C CN100542663 C CN 100542663C CN B2006101695554 A CNB2006101695554 A CN B2006101695554A CN 200610169555 A CN200610169555 A CN 200610169555A CN 100542663 C CN100542663 C CN 100542663C
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- 230000005291 magnetic effect Effects 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims description 14
- 238000009826 distribution Methods 0.000 claims description 9
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 24
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- 238000010521 absorption reaction Methods 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 9
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- 238000006243 chemical reaction Methods 0.000 description 5
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- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 4
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Abstract
本发明提供了一种永磁体旋转搅拌装置,包括内部装有磁性离子液体(10)的密闭容器(4),且容器(4)底部中心设有向内突起的中心磁体凹槽(19),一位于所述中心磁体凹槽(19)内的第一永磁体(5),以及带动第一永磁体(5)在中心磁体凹槽(9)内转动的旋转马达(6),其特征在于,所述容器(4)底部还设有至少一个圆环形磁体凹槽,和至少一个位于所述圆环形磁体凹槽内、可以在旋转马达(6)带动下沿所述圆环形磁体凹槽转动的第二永磁体(22),并且所述第二永磁体(22)的磁极方向与第一永磁体(5)相同;本发明克服了现有永磁体旋转搅拌装置中磁性离子液体因为与永磁体距离增大造成磁力降低,而使旋转动力降低的缺陷。
The invention provides a permanent magnet rotating stirring device, comprising a closed container (4) with a magnetic ionic liquid (10) inside, and the center of the bottom of the container (4) is provided with an inwardly protruding central magnet groove (19), A first permanent magnet (5) located in the central magnet groove (19), and a rotary motor (6) that drives the first permanent magnet (5) to rotate in the central magnet groove (9), is characterized in that , the bottom of the container (4) is also provided with at least one circular magnet groove, and at least one is located in the circular magnet groove, which can be driven by the rotating motor (6) along the circular magnet. The second permanent magnet (22) that groove rotates, and the magnetic pole direction of described second permanent magnet (22) is identical with first permanent magnet (5); The present invention overcomes the magnetic ionic liquid in existing permanent magnet rotating stirring device The defect that the rotational power is reduced due to the decrease of the magnetic force due to the increase of the distance from the permanent magnet.
Description
技术领域 technical field
本发明涉及一种搅拌装置,具体地说是一种磁性离子液体作为介质的永磁体旋转搅拌装置。The invention relates to a stirring device, in particular to a permanent magnet rotating stirring device with a magnetic ionic liquid as a medium.
技术背景 technical background
磁稳定床是针对磁性催化剂的应用而研究的气液反应器,即在反应器外部加上几组固定线圈,当电流通过线圈时产生磁场,磁性催化剂颗粒在磁场的作用下呈规律排列,对反应器中的气泡有破碎切割作用,磁性颗粒催化剂不会随反应介质高速流动而被带出反应器而流失,同时可以利用磁场对磁性催化剂进行回收。磁稳定床在工业上已经取得令人满意的效果,对处理量为70kt的己内酰胺加氢精制过程显示出它的优越性。与工业上常用的连续搅拌釜相比,体积由10m3下降为1.8m3,而且生产质量大幅度提高。但是因为磁场在反应器内部的分布不均匀,磁场随反应器外壁到中心的距离的平方成反比衰减,造成气体分布不均匀,中心磁场低,磁颗粒的浓度低于反应器内壁附近的浓度,故气泡会向中心汇集,同时产生凝并,使气体的利用率降低。为此,又开发了新型的磁反应器,在反应器外加上线圈,当通电时会产生一个旋转磁场,使反应器内部的磁颗粒成自转状态,很大程度上改变气泡分布和液体流动状态。但此研究仍处于小型阶段,尚未放大和工业应用。The magnetically stabilized bed is a gas-liquid reactor researched for the application of magnetic catalysts. That is, several sets of fixed coils are added outside the reactor. When the current passes through the coils, a magnetic field is generated, and the magnetic catalyst particles are arranged regularly under the action of the magnetic field. The bubbles in the reactor have the effect of breaking and cutting, and the magnetic particle catalyst will not be taken out of the reactor with the high-speed flow of the reaction medium and lost. At the same time, the magnetic catalyst can be recovered by using the magnetic field. The magnetically stabilized bed has achieved satisfactory results in the industry, and its superiority has been shown in the hydrofining process of caprolactam with a treatment capacity of 70kt. Compared with the continuous stirring tank commonly used in industry, the volume is reduced from 10m 3 to 1.8m 3 , and the production quality is greatly improved. However, because the distribution of the magnetic field inside the reactor is uneven, the magnetic field attenuates inversely proportional to the square of the distance from the outer wall of the reactor to the center, resulting in uneven gas distribution, a low central magnetic field, and a concentration of magnetic particles lower than that near the inner wall of the reactor. Therefore, the bubbles will gather to the center, and at the same time, condensation will occur, which will reduce the utilization rate of the gas. For this reason, a new type of magnetic reactor has been developed, and a coil is added outside the reactor. When energized, a rotating magnetic field will be generated to make the magnetic particles inside the reactor rotate, which greatly changes the distribution of bubbles and the state of liquid flow. . But this research is still in a small stage and has not yet been scaled up and applied industrially.
离子液体(ionic liquids)是在室温及相邻温度下呈液态的物质,由不对称的有机阳离子和有机或无机阴离子组成。常见的离子液体有疏水性离子液体[bmim]PF6,亲水性离子液体[bmim]BF4,[bmim]Cl等。离子液体具有污染少,毒害小,溶解能力强,挥发性低,热稳定性强,结构可调,回收容易等优点,是新型的绿色溶剂,在许多气体吸收、萃取等方面有广泛的应用。Ionic liquids are substances that are liquid at room temperature and adjacent temperatures, and are composed of asymmetric organic cations and organic or inorganic anions. Common ionic liquids include hydrophobic ionic liquid [bmim]PF 6 , hydrophilic ionic liquid [bmim]BF 4 , [bmim]Cl, etc. Ionic liquids have the advantages of less pollution, less toxicity, strong solubility, low volatility, strong thermal stability, adjustable structure, and easy recovery. They are new green solvents and are widely used in the absorption and extraction of many gases.
磁性离子液体是一种特殊的物质,近年来,日本Hayashi等发现将亲水性离子液体[bmim]Cl与FeCl3·6H2O或FeCl3在N2环境下混合即可得疏水的[bmim]FeCl4,这种离子液体能够强烈的感应磁场,具有顺磁性(Chem.Lett.,Vo1.33,1590~1591,2004)。Magnetic ionic liquid is a special substance. In recent years, Japan’s Hayashi et al. found that the hydrophobic [bmim]Cl can be obtained by mixing the hydrophilic ionic liquid [bmim]Cl with FeCl 3 6H 2 O or FeCl 3 in N 2 environment. ]FeCl 4 , this ionic liquid can strongly sense magnetic fields and has paramagnetism (Chem. Lett., Vo1.33, 1590-1591, 2004).
在名称为“带有旋转、稳定磁力搅拌的萃取装置及其操作方法”的中国专利申请(申请号:200610089480.9)中,披露了一种具有磁性功能的疏水性离子液体作为萃取剂的磁性搅拌分散体系的萃取装置,该装置包括一底部中间部位为向内凹的反应罐,在凹槽里有一与旋转马达的轴相连接的立式圆形钕铁硼永磁铁;在反应罐的下部一侧的壁上开有磁性离子液体出口,另一侧的壁上开有磁性离子液体进口和料液进口,在反应器上部的外侧壁上安装有磁稳定床线圈;在反应器里,一环形分布器的进液口与该料液进口相对接;磁稳定床线圈控制处于分散相的磁性离子液体液珠的相互碰撞、凝并;然而,该装置的反应罐中的磁场随着与永磁铁距离的增加,成平方衰减,造成了反应罐中的磁场分布不均,磁力降低,从而造成旋转动力降低。In the Chinese patent application (application number: 200610089480.9) titled "Extraction Device with Rotating and Stable Magnetic Stirring and Its Operation Method", a magnetically agitated dispersing method using a magnetically functional hydrophobic ionic liquid as an extractant is disclosed. The extraction device of the system includes a reaction tank whose bottom middle part is concave inward, and there is a vertical circular NdFeB permanent magnet connected with the shaft of the rotating motor in the groove; on the lower side of the reaction tank A magnetic ionic liquid outlet is opened on the wall of the reactor, a magnetic ionic liquid inlet and a feed liquid inlet are opened on the wall on the other side, and a magnetically stable bed coil is installed on the outer wall of the upper part of the reactor; in the reactor, a circular distribution The liquid inlet of the device is connected to the feed liquid inlet; the magnetically stable bed coil controls the mutual collision and condensation of the magnetic ionic liquid droplets in the dispersed phase; however, the magnetic field in the reaction tank of the device increases with the distance from the permanent magnet. The increase of , attenuated by the square, caused the uneven distribution of the magnetic field in the reaction tank, the magnetic force decreased, and the rotational power decreased.
发明内容 Contents of the invention
本发明的目的是克服上述现有永磁体旋转搅拌装置中磁性离子液体因为与永磁体距离增大造成磁力降低,而使旋转动力降低的缺陷,从而提供一种永磁体旋转搅拌装置。The purpose of the present invention is to overcome the defect that the magnetic force of the magnetic ionic liquid in the existing permanent magnet rotating stirring device decreases due to the increase of the distance from the permanent magnet, thereby reducing the rotational power, thereby providing a permanent magnet rotating stirring device.
本发明提供的一种永磁体旋转搅拌装置,包括内部装有磁性离子液体10的密闭容器4,且所述容器4底部中心设有向容器4内突起的中心磁体凹槽19,一位于所述中心磁体凹槽19内的第一永磁体5,以及带动第一永磁体5在中心磁体凹槽19内转动的旋转马达6,其特征在于,所述容器4底部还设有至少一个向容器4内突起的圆环形磁体凹槽,和至少一个位于所述圆环形磁体凹槽内、可以在旋转马达6带动下沿所述圆环形磁体凹槽转动的第二永磁体22,并且所述第二永磁体22的磁极方向与第一永磁体5相同。A permanent magnet rotary stirring device provided by the present invention comprises a closed container 4 with a magnetic ionic liquid 10 inside, and the center of the bottom of the container 4 is provided with a
进一步地,上述装置中,所述容器4内的底部还设有至少一个环形气体分布器,所述环形气体分布器为圆环形中空管,其进气口通过气路与容器4的气体入口连通,并且所述环形气体分布器壁上设有至少一个孔洞作为气体分布孔15。Further, in the above device, the bottom of the container 4 is also provided with at least one annular gas distributor, the annular gas distributor is a circular hollow tube, and its air inlet passes through the gas path and the gas in the container 4. The inlet is connected, and at least one hole is provided on the wall of the annular gas distributor as a gas distribution hole 15 .
进一步地,所述环形气体分布器的圆心位于所述容器4的底部中心位置。Further, the center of the annular gas distributor is located at the center of the bottom of the container 4 .
进一步地,所述圆环形磁体凹槽以中心磁体凹槽19为中心。Further, the circular magnet groove is centered on the
进一步地,所述永磁体为钕铁硼永磁体,磁场强度为1000一3000奥斯特。Further, the permanent magnet is an NdFeB permanent magnet, and the magnetic field strength is 1000-3000 Oersted.
进一步地,所述旋转马达6的转速小于300转/分钟。Further, the rotating speed of the rotating motor 6 is less than 300 rpm.
进一步地,所述磁性离子液体10为[bmim]FeCl4。Further, the magnetic ionic liquid 10 is [bmim]FeCl 4 .
磁性离子液体[bmim]FeCl4的合成方法为:等摩尔FeCl3·6H2O或FeCl3与离子液体[bmim]Cl在氮气环境下混合,产生磁性离子液体[bmim]FeCl4(Chem.Lett.,Vol.33,1590~1591,2004)。The synthesis method of magnetic ionic liquid [bmim]FeCl 4 is as follows: equimolar FeCl 3 6H 2 O or FeCl 3 and ionic liquid [bmim]Cl are mixed under nitrogen atmosphere to produce magnetic ionic liquid [bmim]FeCl 4 (Chem.Lett ., Vol.33, 1590-1591, 2004).
本发明的优点如下:The advantages of the present invention are as follows:
1.采用多个永磁体进行旋转搅拌,克服了现有永磁体旋转搅拌装置中磁性离子液体因为与永磁体距离增大造成磁力降低,而使旋转动力降低的缺陷;1. Multiple permanent magnets are used for rotating stirring, which overcomes the defect that the magnetic force of the magnetic ionic liquid in the existing permanent magnet rotating stirring device decreases due to the increase of the distance from the permanent magnet, which reduces the rotational power;
2.使用顺磁性的磁性离子液体,采用旋转磁场,底部采用永磁体提供旋转磁场搅拌,设备底部有环流扰动,并逐渐带动整个磁性离子液体转动,促进溶质在吸收剂中的分散,加快吸收速率;2. Use paramagnetic magnetic ionic liquid, adopt rotating magnetic field, use permanent magnet at the bottom to provide rotating magnetic field stirring, there is circulation disturbance at the bottom of the equipment, and gradually drive the entire magnetic ionic liquid to rotate, promote the dispersion of solute in the absorbent, and accelerate the absorption rate ;
3.以顺磁性的磁性离子液体为吸收剂,采用本发明的磁体旋转搅拌装置制成的吸收装置,避免了传统挥发性有机溶剂的使用,实验表明,磁性离子液体的饱和蒸汽压几乎为零。3. With the paramagnetic magnetic ionic liquid as the absorbent, the absorption device made by the magnet rotating stirring device of the present invention avoids the use of traditional volatile organic solvents. Experiments show that the saturated vapor pressure of the magnetic ionic liquid is almost zero .
4.磁体与吸收体系隔离,避免与体系内物质的直接接触,在高压吸收过程中容易实现体系的密闭;4. The magnet is isolated from the absorption system to avoid direct contact with the substances in the system, and it is easy to realize the airtightness of the system during the high-pressure absorption process;
5.使用永磁铁对磁性离子液体搅拌,剪切力低,适用于含有生物活性物质的体系;5. Using a permanent magnet to stir the magnetic ionic liquid, the shear force is low, and it is suitable for systems containing biologically active substances;
6.永磁体搅拌所需电量更低,电机调速功率比搅拌桨更小,功率远远低于常规搅拌装置,大大减少了过程能耗。6. The permanent magnet stirring requires less electricity, and the motor speed regulation power is smaller than that of the stirring paddle, and the power is far lower than that of the conventional stirring device, which greatly reduces the energy consumption of the process.
附图说明 Description of drawings
图1测量磁性离子液体对苯的吸收能力的测量系统示意图;Fig. 1 measures the schematic diagram of the measurement system of the absorption capacity of magnetic ionic liquid to benzene;
图2a永磁体旋转搅拌装置容器底部示意图;The schematic diagram of the bottom of the container of the permanent magnet rotating stirring device of Fig. 2a;
图2b环形气体分布器示意图;Figure 2b schematic diagram of the annular gas distributor;
图3磁性离子液体对苯蒸汽的吸收曲线图。Fig. 3 The absorption curve of magnetic ionic liquid to benzene vapor.
附图标记reference sign
1、氮气钢瓶 2、气体流量计 3、溶质储罐1.
4、容器 5、第一永磁体 6、旋转马达4.
7、第一环形气体分布器 8、磁体连接轴 9、第二环形气体分布器7. The first annular gas distributor 8. The
10、磁性离子液体 11、第三环形气体分布器 12、气体出口10. Magnetic ionic liquid 11. Third
13、液氮冷阱 14、真空泵 15、气体分布孔13. Liquid
18、第二环形磁体凹槽 19、中心磁体凹槽 20、第一环形磁体凹槽18. Second
22、第二永磁体 23、第三永磁体 24、第四永磁体22. The second
25、第五永磁体 26、第三气路 27、第一气路25. The fifth
28、第二气路28. The second gas path
具体实施方式 Detailed ways
下面结合具体实施例对本发明做进一步的解释和说明。The present invention will be further explained and illustrated below in conjunction with specific embodiments.
如图1所示的测量磁性离子液体对苯蒸汽吸收的系统,采用了本发明的永磁体旋转搅拌装置,氮气钢瓶1通过第一气路27连接至溶质储罐3底部,所述第一气路上设置有气体流量计2,溶质储罐3上部通过第二气路28分别连接至第一、第二和第三环形气体分布器7、9、11,所述第一、第二和第三环形气体分布器7、9、11固定于圆柱筒形容器4内的底部,且同心放置,如图2b和图2a所示,所述容器4底部除中心位置有一个用来容纳第一永磁体5的中心磁体凹槽19外,还设有两个以中心磁体凹槽19为中心的第一和第二环形磁体凹槽20、18,磁体连接轴8上以第一永磁体5为中心分别对称固定第二和第三永磁体22、23,以及第四和第五永磁体24、25,并且第一永磁体5安装在中心磁体凹槽19内,第二和第三永磁体22、23安装在第一环形磁体凹槽内,第四和第五永磁体24、25安装在第二环形凹槽内,五个永磁体都为立式圆柱钕铁硼永磁体,磁场强度为1000—3000奥斯特;旋转马达6可以带动磁体连接轴8绕着圆柱筒形容器4的轴心转动,从而使得固定在其上的五个立式圆柱钕铁硼永磁体在各自的磁体凹槽内转动,达到旋转磁场的目的,旋转马达6的转速小于300转/分钟;容器4的侧壁上部设有气体出口12,并通过第三气路26连接至液氮冷阱13的入口,所述液氮冷阱13的出口与真空泵14连接。As shown in Figure 1, the system for measuring the absorption of benzene vapor by magnetic ionic liquids adopts the permanent magnet rotating stirring device of the present invention, and the nitrogen cylinder 1 is connected to the bottom of the solute storage tank 3 through the first gas path 27, and the first gas A gas flowmeter 2 is arranged on the road, and the upper part of the solute storage tank 3 is respectively connected to the first, second and third annular gas distributors 7, 9, 11 through the second gas passage 28, and the first, second and third Annular gas distributors 7, 9, 11 are fixed to the bottom of the cylindrical container 4 and placed concentrically, as shown in Figure 2b and Figure 2a, the bottom of the container 4 except for the central position has one for accommodating the first permanent magnet Outside the center magnet groove 19 of 5, also be provided with two first and second annular magnet grooves 20,18 centered on the center magnet groove 19, the first permanent magnet 5 is centered on the magnet connecting shaft 8 respectively The second and third permanent magnets 22,23 are fixed symmetrically, and the fourth and fifth permanent magnets 24,25, and the first permanent magnet 5 is installed in the central magnet groove 19, and the second and third permanent magnets 22,23 Installed in the first annular magnet groove, the fourth and fifth permanent magnets 24, 25 are installed in the second annular groove, the five permanent magnets are all vertical cylindrical NdFeB permanent magnets, and the magnetic field strength is 1000-3000 Oster; the rotary motor 6 can drive the magnet connection shaft 8 to rotate around the axis of the cylindrical container 4, so that the five vertical cylindrical NdFeB permanent magnets fixed on it rotate in their respective magnet grooves , to achieve the purpose of rotating the magnetic field, the rotating speed of the rotating motor 6 is less than 300 rpm; the upper part of the side wall of the container 4 is provided with a gas outlet 12, and is connected to the inlet of the liquid nitrogen cold trap 13 through the third gas path 26, the liquid nitrogen The outlet of nitrogen cold trap 13 is connected with vacuum pump 14.
采用上述系统测量磁性离子液体对苯蒸汽吸收的步骤如下:The steps of using the above system to measure the absorption of benzene vapor by magnetic ionic liquid are as follows:
1.将10ml磁性离子液体[bmim]FeCl4置于容器4中;开启真空泵14,待真空度达到10-5Pa后,停止真空泵14;1. Put 10ml of magnetic ionic liquid [bmim]FeCl 4 in the container 4; turn on the
2.启动旋转马达6,调整转数分别为0、7.5转/分钟、12转/分钟和17转/分钟;2. Start the rotary motor 6, and adjust the number of revolutions to be 0, 7.5 revolutions/minute, 12 revolutions/minute and 17 revolutions/minute;
3.开启氮气瓶1,调整流量为80ml/min,氮气作为载气将溶质储罐3内苯的挥发气经第一、第二和第三环形气体分布器7、9、11带入磁性离子液体10,在不同吸收时间下称量液氮冷阱13冷凝出的液态苯的质量以及溶质储罐3中苯减少的质量,计算出不同时间内磁性离子液体10对苯蒸汽的吸收曲线和饱和吸收量,如图3曲线所示。3. Turn on the nitrogen bottle 1, adjust the flow rate to 80ml/min, nitrogen is used as the carrier gas to bring the volatile gas of benzene in the
本发明的永磁体旋转搅拌装置,可以用于吸收装置,也可以用以磁性离子液体为介质的萃取等反应过程中,另外,实施例1采用了两个圆环形磁体凹槽,每个圆环形磁体凹槽内对称设置2个永磁体的方式,根据容器的大小,也可以使用更多的圆环形磁体凹槽或者只使用一个圆环形磁体凹槽;每个圆环形磁体凹槽内可以只设有1个,也可以设置2个、3个、甚至更多个永磁体,来进一步增加磁场强度和均匀性,并且所有永磁体的N极朝同一方向设置,具体到上述实施例1,就是图1中第一至第五永磁体的N极全部朝上或者全部朝下。The permanent magnet rotating stirring device of the present invention can be used in an absorption device, and can also be used in reaction processes such as extraction with a magnetic ionic liquid as a medium. In addition, Embodiment 1 has adopted two circular magnet grooves, each circular Two permanent magnets are arranged symmetrically in the ring magnet groove, and according to the size of the container, more ring magnet grooves or only one ring magnet groove can be used; each ring magnet groove Only one, or two, three, or even more permanent magnets can be set in the slot to further increase the magnetic field strength and uniformity, and the N poles of all permanent magnets are set in the same direction, specific to the above implementation Example 1 is that the N poles of the first to fifth permanent magnets in Fig. 1 are all facing up or all facing down.
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CN2158010Y (en) * | 1991-06-23 | 1994-03-02 | 新环技术开发有限公司 | Sealed magnetic coupling stirrer |
CN2223137Y (en) * | 1994-10-24 | 1996-03-27 | 盐城工业专科学校 | Magnetic stirring machine |
WO2006018560A1 (en) * | 2004-07-08 | 2006-02-23 | Commissariat A L'energie Atomique | Drop microreactor |
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CN2158010Y (en) * | 1991-06-23 | 1994-03-02 | 新环技术开发有限公司 | Sealed magnetic coupling stirrer |
CN2223137Y (en) * | 1994-10-24 | 1996-03-27 | 盐城工业专科学校 | Magnetic stirring machine |
WO2006018560A1 (en) * | 2004-07-08 | 2006-02-23 | Commissariat A L'energie Atomique | Drop microreactor |
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